CN107827117B - Preparation method of multimodal distribution spherical silicon dioxide micro powder - Google Patents
Preparation method of multimodal distribution spherical silicon dioxide micro powder Download PDFInfo
- Publication number
- CN107827117B CN107827117B CN201711176711.4A CN201711176711A CN107827117B CN 107827117 B CN107827117 B CN 107827117B CN 201711176711 A CN201711176711 A CN 201711176711A CN 107827117 B CN107827117 B CN 107827117B
- Authority
- CN
- China
- Prior art keywords
- product
- spheroidizing
- silicon dioxide
- mixing
- mixer
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/51—Particles with a specific particle size distribution
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
Abstract
The invention relates to a preparation method of multimodal distribution spherical silicon dioxide micro powder, which comprises the following steps: selecting silicon dioxide micropowder with purity of more than 99.8% and granularity of 0.1-60 μm as raw material; in a spheroidizing furnace, a flame zone formed by burning natural gas and oxygen is taken as a spheroidizing zone, and the raw materials are introduced into the spheroidizing zone to be spheroidized to obtain a product A, a product B, a product C and a product D; and (3) mixing the product A and the product B according to a mass ratio of 0.1-1: 1, mixing by a high-efficiency mixer, and marking a product after uniform mixing as a product AB; and mixing the product AB, the product C and the product D in a mixer for 10-50 min, and uniformly mixing to obtain the product. The spherical silicon dioxide micropowder prepared by the method at least contains three peaks, and shows the characteristics of good fluidity, large filling amount, low thermal expansion coefficient, low warpage and the like of the filler in plastic packaging material products.
Description
Technical Field
The invention relates to a preparation method of spherical silicon dioxide micro powder, in particular to a preparation method of multimodal distribution spherical silicon dioxide micro powder.
Background
In order to meet the requirements of current consumers on light weight, small size, thinness and the like of end products, the packaging form of the semiconductor industry is changed greatly, the packaging forms of the semiconductor industry are developed from the packaging forms of leaded DIP, SIP and the like to the packaging forms of surface-mounted SOP, TSOP, SSOP, QFP and the like, and the packaging forms of the semiconductor industry are developed towards the packaging forms of underfil and the like.
In the aspect of raising higher requirements on product performance, one of the key performance indexes is the spiral fluidity of the epoxy plastic package material, and generally, the longer the spiral fluidity is, the better the spiral fluidity is. The performance index is closely related to the filler (silicon micropowder), and the proper filler plays a role in determining the flowability of the epoxy molding compound. In order to meet the requirements, firstly, the filler is spheroidized to provide the filling amount and the fluidity of the filler, and secondly, the filler with the multi-peak distribution is prepared. On the other hand, low cost is also a key factor for entry into the market. Under the requirements of the conditions, a spherical silicon dioxide micro powder product with low cost and high performance for packaging medium and high-end semiconductors is prepared.
Patent No. CN 101743198A, applicant's electric chemical industry co, has a disadvantage in that it adds metal silicon powder to the raw material of fine silica powder to prepare multimodal spherical silica. Firstly, because the furnace temperature is too high in the spheroidizing process, ultrafine powder is easy to agglomerate (the patent number of Japanese patent laid-open No. 2-296711, spherical silicon microparticles and a preparation method thereof show that when the temperature is higher than 1300 ℃, the spheroidizing process is easy to fuse, agglomeration is caused, ultrafine powder is difficult to obtain), and the production process is difficult to control; secondly, the content of the superfine spherical powder required by different products is different, so that the spheroidized product cannot be accurately adjusted and cannot be prepared into products with different requirements; thirdly, the metal silicon powder has potential safety hazard, so that safety accidents are easily caused; and fourthly, the metal silicon is a conductive material, the process control is not accurate, and the metal silicon can easily enter products, so that the electrical property of downstream products is failed.
The patent No. CN 103665775B applicant, Wuxi Chundao electronics, Inc. utilizes spherical silica powder, crystalline silica powder, fused silica powder and fumed silica with different particle sizes to prepare multimodal fillers to prepare plastic packaging materials with higher filling amount and better fluidity. The defects are that the added fumed silica has large specific surface area and high oil absorption rate, so that the viscosity of the plastic packaging material is increased rapidly, and the fumed silica cannot be used for packaging products such as SOP (silicon on insulator) and the like.
The patent No. CN 104194274A applicant Jiangsu alli new materials GmbH utilizes two raw materials to grind twice to prepare the bimodal horn-shaped silicon micro powder, and the product produced by the method can not reach the peak value of 0-1 μm. The requirements of package products such as SOP and the like cannot be met.
Disclosure of Invention
The invention aims to solve the technical problem in the prior art and provides a preparation method of spherical silicon dioxide micropowder with good fluidity, low thermal expansion coefficient and low warpage.
The technical problem to be solved by the invention is realized by the following technical scheme, and the invention discloses a preparation method of multimodal distribution spherical silicon dioxide micro powder, which is characterized by comprising the following steps of: the method comprises the following steps:
(1) raw materials: selecting silicon dioxide micropowder with purity of more than 99.8% and granularity of 0.1-60 μm as raw material;
(2) in a spheroidizing furnace, a flame zone formed by burning natural gas and oxygen is used as a spheroidizing zone, and raw materials are introduced into the spheroidizing zone for spheroidizing to obtain the material: d50=0.1 μm-0.5 μm product a, D50=0.6 μm-3.0 μm product B, D50=4 μm-14 μm product C and D50=15 μm-60 μm product D;
(3) and (3) mixing the product A and the product B according to a mass ratio of 0.1-1: 1, mixing by a high-efficiency mixer for 3-30 min, and recording a product after uniform mixing as a product AB;
(4) the mass ratio of the product AB to the product C to the product D is 0.05-0.30: 0.11-0.24: 0.66-1.08, mixing in a mixer for 10-50 min, and uniformly mixing to obtain the product.
The preparation method of the multimodal distribution spherical silicon dioxide micropowder comprises the following steps: the high-efficiency mixer is an air flow mixer, an intensive mixer, a planetary mixer or a homogenizer.
The preparation method of the multimodal distribution spherical silicon dioxide micropowder comprises the following steps: when the high-efficiency mixer is an air flow mixer, the pressure of compressed air is 0.3-2.0 Mpa, and the loading coefficient is 0.3-0.5.
The preparation method of the multimodal distribution spherical silicon dioxide micropowder comprises the following steps: the mixer is a two-dimensional mixer, a three-dimensional mixer, a V-shaped mixer, a double-cone mixer, a non-gravity mixer, a conical mixer or a coulter mixer.
The preparation method of the multimodal distribution spherical silicon dioxide micropowder comprises the following steps: the consumption of the natural gas in the spheroidizing furnace is 0.5 m per kilogram of the silicon micropowder3-2.5m3。
D50 indicates the particle size corresponding to a cumulative volume fraction of a powder of 50%.
Compared with the prior art, the method is simple, products with different grain diameters are prepared by spheroidizing through a flame balling method, the products with different grain diameters are prepared by mixing, and the spherical silicon dioxide micropowder prepared by the method at least contains three peaks and shows the characteristics of good fluidity, large filling amount, low thermal expansion coefficient, low warping and the like of the filler in the plastic package material product.
Drawings
FIG. 1 is a graph showing the particle size distribution of the product obtained in example 4.
FIG. 2 is a graph showing the particle size distribution of the product obtained in example 5.
FIG. 3 is a graph showing the particle size distribution of the product obtained in comparative example 1.
FIG. 4 is a graph showing the particle size distribution of the product obtained in comparative example 2.
Detailed Description
The following further describes particular embodiments of the present invention to facilitate further understanding of the present invention by those skilled in the art, and does not constitute a limitation to the right thereof.
Example 1, a process for the preparation of a multimodal spherical microsilica, comprising the steps of:
(1) raw materials: selecting silicon dioxide micropowder with purity of more than 99.8% and granularity of 0.1-60 μm as raw material;
(2) in a spheroidizing furnace, a flame zone formed by burning natural gas and oxygen is used as a spheroidizing zone, and raw materials are introduced into the spheroidizing zone for spheroidizing to obtain the material: d50=0.1 μm-0.5 μm product a, D50=0.6 μm-3.0 μm product B, D50=4 μm-14 μm product C and D50=15 μm-60 μm product D;
(3) and (3) mixing the product A and the product B according to a mass ratio of 0.1-1: 1, mixing for 3-30 min by using an airflow mixer, wherein the pressure of compressed air of the airflow mixer is 0.3-2.0 Mpa, the loading coefficient is 0.3-0.5, and a product after uniform mixing is marked as a product AB;
(4) the mass ratio of the product AB to the product C to the product D is 0.05-0.30: 0.11-0.24: 0.66-1.08, mixing in a mixer for 10-50 min, and uniformly mixing to obtain the product.
Example 2, in a method for preparing a multimodal spherical fine silica powder according to example 1, the mixer is a two-dimensional mixer, a three-dimensional mixer, a V-type mixer, a double-cone type mixer, a non-gravity mixer, a conical mixer or a coulter type mixer.
Example 3. Process for the preparation of multimodal spherical microsilica according to example 1, the natural gas is used in the nodularisation furnace in an amount of 0.5 m/kg microsilica3-2.5m3。
the mass ratio of the product A to the product B is 0.2: 1, mixing for 10min in an air flow type mixer, wherein the air pressure of the air flow type mixer is 1.2Mpa, the loading coefficient is 0.4, and the mixed product is marked as a product AB. And (3) putting the product AB, the product C and the product D into a two-dimensional mixer according to the mass ratio of 0.10:0.20:0.87, and mixing for 15 minutes, wherein the rotating speed of the two-dimensional mixer is 12rpm, so as to obtain the product. The particle size distribution diagram refers to fig. 1. This particle size distribution is present in multimodal form (with 4 peaks).
Example 5, a method for preparing multimodal spherical silica fume, selecting silica fume with purity of 99.8% or more and particle size of 0.1 μm-60 μm as raw material; in a spheroidizing furnace, a flame zone formed by burning natural gas and oxygen is used as a spheroidizing zone, and the raw materials are introduced into the spheroidizing zone to be spheroidized by different spheroidizing processes to prepare the material: d50=0.1 μm-0.5 μm product a, D50=0.6 μm-3.0 μm product B, D50=4 μm-14 μm product C and D50=15 μm-60 μm product D;
the mass ratio of the product A to the product B is 0.8: 1, mixing for 10min in an air flow mixer, wherein the air pressure of the air flow mixer is 1.9Mpa, the loading coefficient is 0.35, and the mixed product is marked as a product AB. And (3) putting the product AB, the product C and the product D into a two-dimensional mixer according to the mass ratio of 0.08:0.23:0.72, and mixing for 15 minutes, wherein the rotating speed of the two-dimensional mixer is 12rpm, so as to obtain the product. Particle size distribution referring to figure 2, this particle size distribution again contains 4 peaks.
Comparative example 1:
a product B and a product D were obtained by using the method of example 4 or 5, and the product B and the product D were put into a two-dimensional mixer at a mass ratio of 0.10:0.90 and mixed for 15 minutes at a rotation speed of 12rpm to obtain a product having a particle size distribution pattern shown in FIG. 3, which was in a bimodal form.
Comparative example 2:
the product D, i.e., the finished product, obtained by the method of example 4 or 5, has a particle size distribution diagram as shown in FIG. 4, and has only one peak.
The particle size distribution of the product was measured using a Beckman particle sizer.
The product properties of comparative example 1, comparative example 2 and examples 4 and 5 are given in the following table:
From the above data, the overall performance of example 5 is best. That is, the multi-peak spherical silica powder has more excellent performance than that of a single peak (comparative example 2) (or a double peak, comparative example 1), and is mainly characterized by long fluidity, large filling amount, small linear expansion coefficient, high strength and the like.
Claims (1)
1. The preparation method of the spherical silicon dioxide micro powder with multimodal distribution is characterized by comprising the following steps:
selecting silicon dioxide micropowder with purity of more than 99.8% and granularity of 0.1-60 μm as raw material; in a spheroidizing furnace, a flame zone formed by burning natural gas and oxygen is used as a spheroidizing zone, and the raw materials are introduced into the spheroidizing zone to be spheroidized by different spheroidizing processes to prepare the material:
d50=0.1 μm-0.5 μm product a;
d50=0.6 μm-3.0 μm product B;
d50=4 μm-14 μm product C;
and D50=15 μm-60 μm product D;
the mass ratio of the product A to the product B is 0.8: 1, mixing for 10min in an airflow mixer, wherein the air pressure of the airflow mixer is 1.9Mpa, the loading coefficient is 0.35, and the mixed product is marked as a product AB;
and (3) putting the product AB, the product C and the product D into a two-dimensional mixer according to the mass ratio of 0.08:0.23:0.72, and mixing for 15 minutes, wherein the rotating speed of the two-dimensional mixer is 12rpm, so as to obtain the product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711176711.4A CN107827117B (en) | 2017-11-22 | 2017-11-22 | Preparation method of multimodal distribution spherical silicon dioxide micro powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711176711.4A CN107827117B (en) | 2017-11-22 | 2017-11-22 | Preparation method of multimodal distribution spherical silicon dioxide micro powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107827117A CN107827117A (en) | 2018-03-23 |
| CN107827117B true CN107827117B (en) | 2020-12-22 |
Family
ID=61652264
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711176711.4A Active CN107827117B (en) | 2017-11-22 | 2017-11-22 | Preparation method of multimodal distribution spherical silicon dioxide micro powder |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107827117B (en) |
Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2020019277A1 (en) * | 2018-07-27 | 2020-01-30 | 湖州五爻硅基材料研究院有限公司 | Method for preparing spherical powder filler, spherical powder filler prepared thereby and application thereof |
| CN109456620A (en) * | 2018-11-19 | 2019-03-12 | 江苏联瑞新材料股份有限公司 | A kind of low viscosity filler composition and preparation method thereof |
| CN109455726A (en) * | 2018-12-14 | 2019-03-12 | 江苏联瑞新材料股份有限公司 | A kind of preparation method of ball-shaped silicon micro powder used for electronic packaging |
| CN112607756A (en) * | 2020-11-25 | 2021-04-06 | 江苏联瑞新材料股份有限公司 | Preparation method of spherical alumina for epoxy molding and packaging material |
| CN112978740B (en) * | 2021-03-23 | 2023-11-21 | 江苏联瑞新材料股份有限公司 | Preparation method of submicron spherical silica micropowder |
| CN113308229A (en) * | 2021-05-21 | 2021-08-27 | 江苏联瑞新材料股份有限公司 | Preparation method of high-thermal-conductivity spherical powder for ball grid array packaging |
| CN113735149A (en) * | 2021-09-17 | 2021-12-03 | 江苏联瑞新材料股份有限公司 | Preparation method of spherical alumina powder for high-thermal-conductivity underfill |
| CN113881232B (en) * | 2021-11-04 | 2023-03-21 | 广东航迈新材料科技有限公司 | Ceramic organic silica gel material for medium-voltage fire-resistant cable and preparation method thereof |
| CN113929122B (en) * | 2021-11-12 | 2023-09-05 | 联瑞新材(连云港)有限公司 | Preparation method of multimodal distributed high-heat-conductivity alpha-phase spherical alumina |
| CN115368754A (en) * | 2022-08-12 | 2022-11-22 | 吉安豫顺新材料有限公司 | Spherical low-density silica filler |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102020783B (en) * | 2010-10-25 | 2012-05-30 | 武汉大学 | Selection method of fillers for advanced encapsulating material |
| CN105384177B (en) * | 2015-11-27 | 2018-04-13 | 江苏联瑞新材料股份有限公司 | The preparation method of submicron order preparing spherical SiO 2 micro mist |
| CN106335905B (en) * | 2016-08-17 | 2018-08-21 | 江苏联瑞新材料股份有限公司 | The preparation method of high-end copper-clad plate preparing spherical SiO 2 micro mist |
-
2017
- 2017-11-22 CN CN201711176711.4A patent/CN107827117B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN107827117A (en) | 2018-03-23 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107827117B (en) | Preparation method of multimodal distribution spherical silicon dioxide micro powder | |
| KR20160117472A (en) | Agglomerated boron nitride particles, production method for agglomerated boron nitride particles, resin composition including agglomerated boron nitride particles, moulded body, and sheet | |
| JP6902695B2 (en) | Powder magnetic core and mixed soft magnetic powder | |
| CN108250699B (en) | High-thermal-conductivity insulating polybutylene terephthalate alloy and preparation method thereof | |
| JP2008115404A (en) | Flat metal powdery mixture having low coercive force and high permeability, and electromagnetic interference suppressor comprising the flat metal powdery mixture | |
| JP6815087B2 (en) | Spherical eucryptite particles and their manufacturing method | |
| EP3056533A1 (en) | Master batch, master batch group, production method for master batch, and molded synthetic resin article | |
| US10696840B2 (en) | Resin composition for semiconductor encapsulation and semiconductor device | |
| CN116239087A (en) | Ultra-pure low-radioactivity spheroid beta silicon nitride powder, and manufacturing method and application thereof | |
| JP2021059789A (en) | Copper alloy powder for lamination shaping, lamination shaped product production method, and lamination shaped product | |
| JP2008106334A (en) | Flat metal powdery mixture having low coercive force and high permeability, and electromagnetic interference suppressor containing the flat metal powdery mixture | |
| JP2008106335A (en) | Flat metal powdery mixture having low coercive force and high permeability and electromagnetic interference suppressor containing the flat metal powdery mixture | |
| KR101656131B1 (en) | Method of Manufacturing Nano Material from Graphite-Metal Composite by Mechanical Alloying and Collected Nano Material Using the Same | |
| KR102441218B1 (en) | Tungsten Carbide Powder | |
| CN113735149A (en) | Preparation method of spherical alumina powder for high-thermal-conductivity underfill | |
| JP7313195B2 (en) | Method for producing metal powder and method for producing silver-coated metal powder | |
| JP2000319633A (en) | Silica filter for epoxy resin sealing material | |
| JP5993824B2 (en) | Thermally conductive resin composition, method for producing the same, and article | |
| JP2004203664A (en) | Spherical siliceous powder and manufacturing method and utilization of the same | |
| WO2021100807A1 (en) | Method for adjusting particle crush strength of boron nitride powder, boron nitride powder and method for producing same | |
| US10376956B2 (en) | Extrudable mixture for use in 3D printing systems to produce metal, glass and ceramic articles of high purity and detail | |
| CN109836849B (en) | Preparation method of spherical silicon dioxide with high balling rate | |
| JP6312735B2 (en) | Thermally conductive filler for resin | |
| WO2024048663A1 (en) | Aluminum nitride powder and resin composition | |
| JP2000178414A (en) | Spherical silica for semiconductor encapsulant |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |